CA1150222A - Process for producing crystalline type-a zeolite powder - Google Patents
Process for producing crystalline type-a zeolite powderInfo
- Publication number
- CA1150222A CA1150222A CA000371689A CA371689A CA1150222A CA 1150222 A CA1150222 A CA 1150222A CA 000371689 A CA000371689 A CA 000371689A CA 371689 A CA371689 A CA 371689A CA 1150222 A CA1150222 A CA 1150222A
- Authority
- CA
- Canada
- Prior art keywords
- sodium
- minutes
- per litre
- volume
- parts
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
- C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
- C11D3/1246—Silicates, e.g. diatomaceous earth
- C11D3/128—Aluminium silicates, e.g. zeolites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/26—Aluminium-containing silicates, i.e. silico-aluminates
- C01B33/28—Base exchange silicates, e.g. zeolites
- C01B33/2807—Zeolitic silicoaluminates with a tridimensional crystalline structure possessing molecular sieve properties; Isomorphous compounds wherein a part of the aluminium ore of the silicon present may be replaced by other elements such as gallium, germanium, phosphorus; Preparation of zeolitic molecular sieves from molecular sieves of another type or from preformed reacting mixtures
- C01B33/2815—Zeolitic silicoaluminates with a tridimensional crystalline structure possessing molecular sieve properties; Isomorphous compounds wherein a part of the aluminium ore of the silicon present may be replaced by other elements such as gallium, germanium, phosphorus; Preparation of zeolitic molecular sieves from molecular sieves of another type or from preformed reacting mixtures of type A (UNION CARBIDE trade name; corresponds to GRACE's types Z-12 or Z-12L)
- C01B33/2823—Zeolitic silicoaluminates with a tridimensional crystalline structure possessing molecular sieve properties; Isomorphous compounds wherein a part of the aluminium ore of the silicon present may be replaced by other elements such as gallium, germanium, phosphorus; Preparation of zeolitic molecular sieves from molecular sieves of another type or from preformed reacting mixtures of type A (UNION CARBIDE trade name; corresponds to GRACE's types Z-12 or Z-12L) from aqueous solutions of an alkali metal aluminate and an alkali metal silicate excluding any other source of alumina or silica
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S423/00—Chemistry of inorganic compounds
- Y10S423/24—LTA, e.g. A, alpha, ZK-4, ZK-21, ZK-22
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Detergent Compositions (AREA)
- Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)
Abstract
ABSTRACT OF THE DISCLOSURE
A crystalline type-A zeolite powder, which can be used as a phosphate substitute in detergents, is produced by precipitation reaction in that in a defined sequence sodium-tetrasilicate solution and sodium-aluminate liquor are simultaneously passed to a reactor containing water, whereupon sodium-tetrasilicate solution is added first and sodium-aluminate liquor thereafter. The crystalline product has an average particle size of 6.7 to 8 µm and a narrow particle size distribution curve.
A crystalline type-A zeolite powder, which can be used as a phosphate substitute in detergents, is produced by precipitation reaction in that in a defined sequence sodium-tetrasilicate solution and sodium-aluminate liquor are simultaneously passed to a reactor containing water, whereupon sodium-tetrasilicate solution is added first and sodium-aluminate liquor thereafter. The crystalline product has an average particle size of 6.7 to 8 µm and a narrow particle size distribution curve.
Description
~1~222 The present invention relates to a process for producing crystalline type-A zeolite powder having an average particle diameter of 6.7 to 8.0 llm.
Zeolite A is a crystalline alkali metal aluminium si]icate whose composition corresponds to the formula 1-0 ~ 0-2 M2/nO : AQ2O3 : 1.85 - 0.5 SiO2 . y H2O
wherein M represents a metal cation, n is valency and y a value of up to 6.
Zeolite A is increasingly gaining in importance as a phosphate substitute in detergents. For this purpose it is desirable that the crystalline type-A zeolite powder has a particle size as homogeneous as possible, i.e., that is has a particle size distribution curve as narrow as possible.
The present invention provides a process for producing a crystalline type-A zeolite powder having an average particle diameter of 6.7 to 8 ~m. This process is in which during a period of S to 15 minutes while stirring at a temperature of 30 to 70C
Zeolite A is a crystalline alkali metal aluminium si]icate whose composition corresponds to the formula 1-0 ~ 0-2 M2/nO : AQ2O3 : 1.85 - 0.5 SiO2 . y H2O
wherein M represents a metal cation, n is valency and y a value of up to 6.
Zeolite A is increasingly gaining in importance as a phosphate substitute in detergents. For this purpose it is desirable that the crystalline type-A zeolite powder has a particle size as homogeneous as possible, i.e., that is has a particle size distribution curve as narrow as possible.
The present invention provides a process for producing a crystalline type-A zeolite powder having an average particle diameter of 6.7 to 8 ~m. This process is in which during a period of S to 15 minutes while stirring at a temperature of 30 to 70C
2 to 8 parts by volume of sodium-aluminate liquor having a con-centration of 5 to 200 g, preferably 90 to 150 g of Na2O per litre and 30 to 150 g, preferably 100 to 110 g of ~Q23 per litre and 0.6 to 1.2 parts by volume of a sodium tetrasilicate solution having a concentration of 90 to 120 g, preferably 100 to 110 g of Na2O and 330 to 380 g, preferably 340 to 370 g of sio2 per litre, which, when required, can be diluted with 1.0 to 1.5 parts by volume of water, are simultaneously passed into a reactor containing 8 to 12 parts by volume of water, the mixture is then stirred for 10 to 40 minutes, whereupon at a temperature of 30 to 70C during a period of 5 to 15 minutes further 2 to 3 parts by volume of sodium-tetrasilicate solution having the same con-centration are added, followed by stirring for a period of 10 to 40 minutes at a temperature of 30 to 70C, thereafter while stirring at a temperature of 30 to 70C further 16 to 20 parts by volume - 1 - ~
~IL54~2~2 of a sodium-aluminate liquor having the same concentration are added during a period of 5 to 15 minutes, the reaction mixture is then stirred over a period of 20 to 180 minutes at a temperature of 75 to 100C, it is cooled and the crystalline product is then filtered off and dried.
The type-A zeolite powder produced by means of the process of the present invention has an average particle diameter of 6.7 to 8.0 ~m and a grit content of <0.025~. It can be used with advantage as a phosphate substitute in detergents.
The process according to the present invention is illustrated and described in greater detail by means of the following Examples:
_xample 1 10 litres of water are put into a reactor. At a tempera-ture of 35C during a period of 10 minutes 2 litres of sodium-aluminium liquor having a concentration of 135 g of Na2O per litre and 78 g of AQ2O3 per litre and 1.2 litres of sodium-tetrasilicate solution having a concentration of 100 g of Na2O per litre and 349 g of SiO2 per litre are then passed simultaneously into this reactor while stirring. The mixture is then stirred for 30 minutes. Yurther, 2.4 litres of sodium tetrasilicate solution having the same concentration are then added during a period of 10 minutes at a temperature of 35C, followed by stirring for further 30 minutes. Thereafter, while stirring at a temperature of 35C, further 18 litres of sodium-aluminate liquor having the same concentration are added during 10 minutes. The reaction mixture is stirred for further 50 minutes at 98C and cooled.
The crystalline reaction product is filtered off and dried.
The particle size distribution curve is determined by means of the Coulter counter and the following values are obtained:
~15~Z;2Z
50% < 8.0 IJm 17~ < 10 ~Im 4% < 15 ~
The grit content (particles >45 1lm) according to Mocker is 0.024~. The calcium binding power is 148 mg of CaO per gram of zeolite.
_xample _ 10 litres of water are put into a reactor. At a temperature of 48C during a period of 10 minutes 2 litres of sodium-aluminate liquor having a concentration of 145 g of Na2O
per litre and 81 g of AQ2O3 per litre and 0.6 litre of sodium-tetrasilicate solution having a concentration of 100 g of Na2O
per litre and 349 g of SiO2 per litre, which is diluted with 1.4 litres of water, are then passed simultaneously into this reactor while stirring. The reaction mixture is then stirred for 30 minutes. Further 3.0 litres of sodium-tetrasilicate solution having the same concentration are then added during a period of 10 minutes at a temperature of 48C. This is followed by stirring for further 30 minutes, whereupon, while stirring at a temperature of 48C, further 18 litres of sodium aluminate liquor having the same concentration are added during 10 minutes. The reaction mixture is then stirred for further 80 minutes at a temperature of 88C and cooled.
The crystalline reaction product is filtered off and dried.
The particle size distribution curve is determined by means of the Coulter counter and the following values are obtained:
50% < 6.7 ~Im 12% < 10 ~m 4% < 15 ~m The grit content (particles >45 ~m) according to Mocker is 0.018~ and the calcium binding power is 151 mg of CaO per gram of zeolite.
~IL54~2~2 of a sodium-aluminate liquor having the same concentration are added during a period of 5 to 15 minutes, the reaction mixture is then stirred over a period of 20 to 180 minutes at a temperature of 75 to 100C, it is cooled and the crystalline product is then filtered off and dried.
The type-A zeolite powder produced by means of the process of the present invention has an average particle diameter of 6.7 to 8.0 ~m and a grit content of <0.025~. It can be used with advantage as a phosphate substitute in detergents.
The process according to the present invention is illustrated and described in greater detail by means of the following Examples:
_xample 1 10 litres of water are put into a reactor. At a tempera-ture of 35C during a period of 10 minutes 2 litres of sodium-aluminium liquor having a concentration of 135 g of Na2O per litre and 78 g of AQ2O3 per litre and 1.2 litres of sodium-tetrasilicate solution having a concentration of 100 g of Na2O per litre and 349 g of SiO2 per litre are then passed simultaneously into this reactor while stirring. The mixture is then stirred for 30 minutes. Yurther, 2.4 litres of sodium tetrasilicate solution having the same concentration are then added during a period of 10 minutes at a temperature of 35C, followed by stirring for further 30 minutes. Thereafter, while stirring at a temperature of 35C, further 18 litres of sodium-aluminate liquor having the same concentration are added during 10 minutes. The reaction mixture is stirred for further 50 minutes at 98C and cooled.
The crystalline reaction product is filtered off and dried.
The particle size distribution curve is determined by means of the Coulter counter and the following values are obtained:
~15~Z;2Z
50% < 8.0 IJm 17~ < 10 ~Im 4% < 15 ~
The grit content (particles >45 1lm) according to Mocker is 0.024~. The calcium binding power is 148 mg of CaO per gram of zeolite.
_xample _ 10 litres of water are put into a reactor. At a temperature of 48C during a period of 10 minutes 2 litres of sodium-aluminate liquor having a concentration of 145 g of Na2O
per litre and 81 g of AQ2O3 per litre and 0.6 litre of sodium-tetrasilicate solution having a concentration of 100 g of Na2O
per litre and 349 g of SiO2 per litre, which is diluted with 1.4 litres of water, are then passed simultaneously into this reactor while stirring. The reaction mixture is then stirred for 30 minutes. Further 3.0 litres of sodium-tetrasilicate solution having the same concentration are then added during a period of 10 minutes at a temperature of 48C. This is followed by stirring for further 30 minutes, whereupon, while stirring at a temperature of 48C, further 18 litres of sodium aluminate liquor having the same concentration are added during 10 minutes. The reaction mixture is then stirred for further 80 minutes at a temperature of 88C and cooled.
The crystalline reaction product is filtered off and dried.
The particle size distribution curve is determined by means of the Coulter counter and the following values are obtained:
50% < 6.7 ~Im 12% < 10 ~m 4% < 15 ~m The grit content (particles >45 ~m) according to Mocker is 0.018~ and the calcium binding power is 151 mg of CaO per gram of zeolite.
- 3
Claims (4)
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. A process for producing a crystalline type-A
zeolite powder having an average particle diameter of 6.7 to 8.0 µm which comprises simultaneously passing over a period of 5 to 15 minutes with stirring at a temperature of 30 to 70°C, 2 to 8 parts by volume of a sodium-aluminate liquor having a con-centration of 50 to 200 g of Na2O per litre and 30 to 100 g of A?2O3 per litre and 0.6 to 1.2 parts by volume of a sodium-tetrasilicate solution having a concentration of 90 to 120 g of Na2O per litre and 330 to 380 g of SiO2 per litre, into a reactor containing 8 to 12 parts by volume of water, followed by stirring for a period of 10 to 40 minutes, then at a temperature of 38 to 70°C over a period of 5 to 15 minutes adding a further 2 to 3 parts by volume of sodium-tetrasilicate solution having the same concentration, followed by stirring for 10 to 40 minutes at a temperature of 30 to 70°C, thereafter, while stirring at a temperature of 30 to 70°C, adding a further 16 to 20 parts by volume of a sodium-aluminate liquor having the same concentration over a period of 5 to 15 minutes stirring the reaction mixture over a period of 20 to 180 minutes at a temperature of 75 to 100°C, and cooling the reaction mixture, the crystalline product is filtered off and dried.
zeolite powder having an average particle diameter of 6.7 to 8.0 µm which comprises simultaneously passing over a period of 5 to 15 minutes with stirring at a temperature of 30 to 70°C, 2 to 8 parts by volume of a sodium-aluminate liquor having a con-centration of 50 to 200 g of Na2O per litre and 30 to 100 g of A?2O3 per litre and 0.6 to 1.2 parts by volume of a sodium-tetrasilicate solution having a concentration of 90 to 120 g of Na2O per litre and 330 to 380 g of SiO2 per litre, into a reactor containing 8 to 12 parts by volume of water, followed by stirring for a period of 10 to 40 minutes, then at a temperature of 38 to 70°C over a period of 5 to 15 minutes adding a further 2 to 3 parts by volume of sodium-tetrasilicate solution having the same concentration, followed by stirring for 10 to 40 minutes at a temperature of 30 to 70°C, thereafter, while stirring at a temperature of 30 to 70°C, adding a further 16 to 20 parts by volume of a sodium-aluminate liquor having the same concentration over a period of 5 to 15 minutes stirring the reaction mixture over a period of 20 to 180 minutes at a temperature of 75 to 100°C, and cooling the reaction mixture, the crystalline product is filtered off and dried.
2. A process according to claim 1, in which the sodium aluminate liquor has a concentration of 90 to 150 g of Na2O per litre and 100 to 110 g of A?2O3 per litre.
3. A process according to claim 2, in which the sodium tetrasilicate has a concentration of 100 to 110 g of Na2O per litre and 340 to 370 g of SiO2 per litre.
4. A process according to claim 1, 2 or 3, in which the sodium tetrasilicate passed with the sodium aluminate is diluted with 1.0 to 1.5 parts by volume of water.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEP3007080.5 | 1980-02-26 | ||
| DE19803007080 DE3007080A1 (en) | 1980-02-26 | 1980-02-26 | METHOD FOR PRODUCING TYPE A CRYSTALLINE ZEOLITE POWDER |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1150222A true CA1150222A (en) | 1983-07-19 |
Family
ID=6095542
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000371689A Expired CA1150222A (en) | 1980-02-26 | 1981-02-25 | Process for producing crystalline type-a zeolite powder |
Country Status (9)
| Country | Link |
|---|---|
| US (1) | US4339419A (en) |
| EP (1) | EP0034696B1 (en) |
| JP (1) | JPS56134515A (en) |
| AT (1) | ATE7378T1 (en) |
| BR (1) | BR8101035A (en) |
| CA (1) | CA1150222A (en) |
| DE (2) | DE3007080A1 (en) |
| ES (1) | ES8201103A1 (en) |
| FI (1) | FI72438C (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE9017906U1 (en) * | 1989-10-06 | 1993-01-21 | Sports Step, Inc., Atlanta, Ga. | Adjustable step structure for aerobic exercises |
| GB2252305A (en) * | 1991-01-31 | 1992-08-05 | Foret Sa | Zeolite manufacture by a continuous gel crystallization process |
| DE4309656A1 (en) * | 1993-03-25 | 1994-09-29 | Henkel Kgaa | Process for the production of very finely divided zeolitic alkali metal aluminum silicates |
| CZ20011894A3 (en) * | 1999-10-26 | 2002-01-16 | Ajkai Timföld Kft | Process for producing synthetic zeolites |
| EP1215277B2 (en) † | 2000-12-18 | 2009-11-25 | Kao Corporation | Base particles and detergent particles |
| US7052541B2 (en) * | 2002-06-19 | 2006-05-30 | Board Of Regents, The University Of Texas System | Color compositions |
| US7425235B2 (en) * | 2005-02-11 | 2008-09-16 | The Board Of Regents Of The University Of Texas System | Color compositions and methods of manufacture |
| KR20080047343A (en) * | 2005-06-17 | 2008-05-28 | 더 보드 오브 리전츠 오브 더 유니버시티 오브 텍사스 시스템 | Organic/inorganic lewis acid composite materials |
| CN104845757B (en) * | 2015-03-30 | 2018-07-06 | 石家庄健达高科化工有限公司 | A kind of method of 4A zeolites slurry production washing powder |
| CN104845760B (en) * | 2015-03-30 | 2018-07-06 | 石家庄健达高科化工有限公司 | A kind of method of the 4A zeolites slurry production washing powder of high-efficiency environment friendly |
Family Cites Families (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AR208392A1 (en) * | 1973-05-07 | 1976-12-27 | Henkel & Cie Gmbh | COMPOSITION TO WASH, WHITE OR CLEAN RESISTANT MATERIALS, ESPECIALLY TEXTILES ADDITIONAL TO PATENT NO 201687 ADDITIONAL TO NO 253286 |
| DE2517218B2 (en) * | 1975-04-18 | 1977-05-05 | Henkel & Cie GmbH, 4000 Düsseldorf; Deutsche Gold- und Silber-Scheideanstalt vormals Roessler, 6000 Frankfurt | TYPE A CRYSTALLINE ZEOLITE POWDER |
| US4041135A (en) * | 1975-07-25 | 1977-08-09 | J. M. Huber Corporation | Production of high capacity inorganic crystalline base exchange materials |
| AT356628B (en) * | 1976-02-06 | 1980-05-12 | Henkel Kgaa | METHOD FOR THE PRODUCTION OF AQUEOUS, FOR FURTHER PROCESSING OF WASHING AND CLEANING AGENTS SUITABLE SUSPENSIONS OF FINE-PARTICULATE WATER-UNLOCATED WATER-UNLOCKED WATER-UNLOCKED |
| DE2651420A1 (en) * | 1976-11-11 | 1978-05-18 | Degussa | TYPE A V CRYSTALLINE ZEOLITE POWDER |
| DE2651485A1 (en) * | 1976-11-11 | 1978-05-24 | Degussa | TYPE A I CRYSTALLINE ZEOLITE POWDER |
| DE2651437A1 (en) * | 1976-11-11 | 1978-05-18 | Degussa | TYPE A VI CRYSTALLINE ZEOLITE POWDER |
| DE2651436A1 (en) * | 1976-11-11 | 1978-05-18 | Degussa | TYPE A III CRYSTALLINE ZEOLITE POWDER |
| DE2651419A1 (en) * | 1976-11-11 | 1978-05-18 | Degussa | TYPE A IV CRYSTALLINE ZEOLITE POWDER |
| DE2705088C2 (en) * | 1977-02-08 | 1986-05-22 | Kali-Chemie Ag, 3000 Hannover | Process for the production of predominantly crystalline sodium aluminum silicates |
| DE2734296A1 (en) * | 1977-07-29 | 1979-02-08 | Degussa | PROCESS FOR THE PRODUCTION OF FINE PARTICULAR, WATER-INSOLUBLE SILICATES ENABLED FOR CATION EXCHANGE |
-
1980
- 1980-02-26 DE DE19803007080 patent/DE3007080A1/en not_active Withdrawn
-
1981
- 1981-01-13 EP EP81100175A patent/EP0034696B1/en not_active Expired
- 1981-01-13 DE DE8181100175T patent/DE3163430D1/en not_active Expired
- 1981-01-13 AT AT81100175T patent/ATE7378T1/en active
- 1981-02-13 FI FI810442A patent/FI72438C/en not_active IP Right Cessation
- 1981-02-20 BR BR8101035A patent/BR8101035A/en unknown
- 1981-02-24 US US06/237,730 patent/US4339419A/en not_active Expired - Fee Related
- 1981-02-25 ES ES499768A patent/ES8201103A1/en not_active Expired
- 1981-02-25 CA CA000371689A patent/CA1150222A/en not_active Expired
- 1981-02-25 JP JP2561181A patent/JPS56134515A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| ES499768A0 (en) | 1981-12-01 |
| JPS56134515A (en) | 1981-10-21 |
| ATE7378T1 (en) | 1984-05-15 |
| JPS6114081B2 (en) | 1986-04-17 |
| EP0034696A1 (en) | 1981-09-02 |
| FI810442L (en) | 1981-08-27 |
| EP0034696B1 (en) | 1984-05-09 |
| BR8101035A (en) | 1981-09-01 |
| FI72438B (en) | 1987-02-27 |
| US4339419A (en) | 1982-07-13 |
| DE3007080A1 (en) | 1981-09-10 |
| FI72438C (en) | 1987-06-08 |
| DE3163430D1 (en) | 1984-06-14 |
| ES8201103A1 (en) | 1981-12-01 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| MKEX | Expiry |